++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ + XPREP - DATA PREPARATION & RECIPROCAL SPACE EXPLORATION Ver. 5.1/NT + + COPYRIGHT(c) 1997 Bruker Analytical X-ray Systems All Rights Reserved + + s92 started at 09:27:29 on 25-MAY-0 + ++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++++ Original cell in Angstroms and degrees: 12.859 10.738 23.112 90.00 93.81 90.00 9730 Reflections read from file s92.hkl; mean (I/sigma) = 7.62 Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4854 4854 0 4869 4854 6482 6493 9730 N (int>3sigma) = 0 3042 3042 0 2799 3042 4294 4286 6397 Mean intensity = 0.0 66.8 66.8 0.0 51.2 66.8 72.0 73.8 71.8 Mean int/sigma = 0.0 7.3 7.3 0.0 6.5 7.3 7.7 7.7 7.7 Lattice type: C chosen Volume: 3184.28 ------------------------------------------------------------------------------- DETERMINATION OF REDUCED (NIGGLI) CELL Transformation from original cell (HKLF-matrix): 0.5000 0.5000 0.0000 0.5000 -0.5000 0.0000 0.0000 0.0000 -1.0000 Unitcell: 8.376 8.376 23.112 87.08 87.08 79.73 Niggli form: a.a = 70.16 b.b = 70.16 c.c = 534.17 b.c = 9.88 a.c = 9.88 a.b = 12.51 ------------------------------------------------------------------------------- SEARCH FOR HIGHER METRIC SYMMETRY ------------------------------------------------------------------------------ Option A: FOM = 0.000 deg. MONOCLINIC C-lattice R(int) = 0.057 [ 5990] Cell: 12.859 10.738 23.112 90.00 93.81 90.00 Volume: 3184.28 Matrix: 1.0000 0.0000 0.0000 0.0000 1.0000 0.0000 0.0000 0.0000 1.0000 Option A selected ------------------------------------------------------------------------------- SPACE GROUP DETERMINATION Lattice exceptions: P A B C I F Obv Rev All N (total) = 0 4854 4854 0 4869 4854 6482 6493 9730 N (int>3sigma) = 0 3042 3042 0 2799 3042 4294 4286 6397 Mean intensity = 0.0 66.8 66.8 0.0 51.2 66.8 72.0 73.8 71.8 Mean int/sigma = 0.0 7.3 7.3 0.0 6.5 7.3 7.7 7.7 7.7 Crystal system M and Lattice type C selected Mean |E*E-1| = 0.962 [expected .968 centrosym and .736 non-centrosym] Chiral flag NOT set Systematic absence exceptions: -c- N 372 N I>3s 1 0.7 0.5 Option Space Group No. Type Axes CSD R(int) N(eq) Syst. Abs. CFOM [A] C2/c # 15 centro 1 3696 0.057 5990 0.5 / 7.7 1.43 [B] Cc # 9 non-cen 1 566 0.057 5990 0.5 / 7.7 6.68 Option [A] chosen ------------------------------------------------------------------------------- Determination of unit-cell contents Formula: C19 H20 N2 S1 O2 Si1 Formula weight = 368.52 Tentative Z (number of formula units/cell) = 6.0 giving rho = 1.153, non-H atomic volume = 21.2 and following cell contents and analysis: C 114.00 61.92 % H 120.00 5.47 % N 12.00 7.60 % O 12.00 8.68 % Si 6.00 7.62 % S 6.00 8.70 % F(000) = 1164.0 Mo-K(alpha) radiation Mu (mm-1) = 0.22 ------------------------------------------------------------------------------- File s92.ins set up as follows: TITL s92 in C2/c CELL 0.71073 12.8588 10.7382 23.1122 90.000 93.811 90.000 ZERR 6.00 0.0026 0.0021 0.0046 0.000 0.030 0.000 LATT 7 SYMM -X, Y, 0.5-Z SFAC C H N O SI S UNIT 114 120 12 12 6 6 TREF HKLF 4 END -------------------------------------------------------------------------------